EP1812348A1 - Procede pour la synthese de nanoparticules de dioxyde de titane - Google Patents

Procede pour la synthese de nanoparticules de dioxyde de titane

Info

Publication number
EP1812348A1
EP1812348A1 EP05807465A EP05807465A EP1812348A1 EP 1812348 A1 EP1812348 A1 EP 1812348A1 EP 05807465 A EP05807465 A EP 05807465A EP 05807465 A EP05807465 A EP 05807465A EP 1812348 A1 EP1812348 A1 EP 1812348A1
Authority
EP
European Patent Office
Prior art keywords
water
tio
titanium
particles
metal
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
EP05807465A
Other languages
German (de)
English (en)
Other versions
EP1812348A4 (fr
Inventor
Insoo Kim
Young Jin Choi
Gang Hyuk Kim
Woo Jin Lee
Charles E. Smith, Jr.
Youg Jin Kim
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Tokusen USA Inc
Original Assignee
Tokusen USA Inc
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Tokusen USA Inc filed Critical Tokusen USA Inc
Publication of EP1812348A1 publication Critical patent/EP1812348A1/fr
Publication of EP1812348A4 publication Critical patent/EP1812348A4/fr
Withdrawn legal-status Critical Current

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G23/00—Compounds of titanium
    • C01G23/04—Oxides; Hydroxides
    • C01G23/047—Titanium dioxide
    • C01G23/053—Producing by wet processes, e.g. hydrolysing titanium salts
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G23/00—Compounds of titanium
    • C01G23/04—Oxides; Hydroxides
    • C01G23/047—Titanium dioxide
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82B—NANOSTRUCTURES FORMED BY MANIPULATION OF INDIVIDUAL ATOMS, MOLECULES, OR LIMITED COLLECTIONS OF ATOMS OR MOLECULES AS DISCRETE UNITS; MANUFACTURE OR TREATMENT THEREOF
    • B82B3/00—Manufacture or treatment of nanostructures by manipulation of individual atoms or molecules, or limited collections of atoms or molecules as discrete units
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G23/00—Compounds of titanium
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G23/00—Compounds of titanium
    • C01G23/04—Oxides; Hydroxides
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G23/00—Compounds of titanium
    • C01G23/04—Oxides; Hydroxides
    • C01G23/047—Titanium dioxide
    • C01G23/053—Producing by wet processes, e.g. hydrolysing titanium salts
    • C01G23/0532—Producing by wet processes, e.g. hydrolysing titanium salts by hydrolysing sulfate-containing salts
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G23/00—Compounds of titanium
    • C01G23/04—Oxides; Hydroxides
    • C01G23/047—Titanium dioxide
    • C01G23/053—Producing by wet processes, e.g. hydrolysing titanium salts
    • C01G23/0536—Producing by wet processes, e.g. hydrolysing titanium salts by hydrolysing chloride-containing salts
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/36—Compounds of titanium
    • C09C1/3607—Titanium dioxide
    • C09C1/3653—Treatment with inorganic compounds
    • C09C1/3661—Coating
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
    • C01P2002/84—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by UV- or VIS- data
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/03—Particle morphology depicted by an image obtained by SEM
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer

Definitions

  • TiO 2 TiO 2
  • metal-doped TiO 2 metal-doped TiO 2
  • metal-coated TiO 2 particles of spherical form factor and needle type of which the average particle size is below 150nm.
  • Titanium dioxide is a material having diverse fields of application such as paints, plastics, cosmetics, inks, paper, chemical fiber, and optical catalysts.
  • TiO 2 is currently being produced all over the world using a sulfate and chloride process, but there is a problem in applying this process in a field that requires ultra-micro characteristics, since this process produces a relatively large particle diameter (sub-micron level) which does not have a high degree of purity.
  • nano-sized TiO 2 As a need for nano-sized TiO 2 increases in diverse fields, a number of researches have been conducted in this field. However, nano-sized TiO 2 is not used extensively due to the high price resulting from the complex production processes now in use. To solve this problem, it is desirable that a production process be developed so that the production cost of nano-sized TiO 2 can be lowered by increased production efficiency in a simplified production process for nano- sized pure T ⁇ O2, metal-doped TiO 2 , and metal-coated TiO 2 .
  • the present invention is a method for synthesizing TiO 2 , metal-doped TiO 2 , and metal-coated TiO 2 particles of spherical form factor and needle type of which the average particle size is below 150nm.
  • the method of the invention is to synthesize Ti(OH) 4 , metal-doped Ti(OH) 4 or metal-coated Ti(OH) 4 , and then react the same by applying a pressure at or above the saturated vapor pressure at a temperature above 10O 0 C.
  • the pressure is achieved by means of the pressure of water vapor generated during the reaction inside of a closed reactor, by pressure applied from the outside, or a mixture of both.
  • Gases to increase the pressure from outside are preferably inert gases such as Ar and N 2 but are not limited to inert gases.
  • Figs. 1 (a)-(b) relate to the TiO 2 powder obtained by the process described in Example 1.
  • Fig 1 ⁇ a) is an FESEM microphotograph.
  • Fig. 1 ⁇ b) is an XRD pattern.
  • Figs. 2(a)-(e) relate to the Ag-doped TiO 2 powder obtained by the process described in Example 2.
  • Fig. 2(a) is an FESEM microphotograph.
  • Fig. 2(b) is an XRD pattern.
  • Fig. 2(c) is an XPS survey scan.
  • Fig. 2(d) is an XPS narrow scan for silver peaks.
  • Fig. 2(e) is a chart of UV-visible absorption.
  • Figs. 1 (a)-(b) relate to the TiO 2 powder obtained by the process described in Example 1.
  • Fig 1 ⁇ a) is an FESEM microphotograph.
  • Fig. 1 ⁇ b) is an XRD pattern.
  • Fig. 3(a)-(c) relate to the Cr-doped TiO 2 powder obtained by the process described in Example 3.
  • Fig. 3(a) is an FESEM microphotograph.
  • Fig. 3(b) is an XRD pattern.
  • Fig. 3(c) is an EDS analysis.
  • Figs. 4(a)-(d) relate to the Ag-coated TiO 2 powder obtained by the process described in Example 4.
  • Fig. 4(a) is an FESEM microphotograph.
  • Fig. 4(b) is an XRD pattern.
  • Fig. 4(c) is an XPS survey scan.
  • Fig. 4(d) is an XPS narrow scan.
  • the object of the present development is to develop a method that synthesizes a large volume of pure TiO 2 , metal-doped TiO 2 , and metal-coated TiO 2 having a primary particle size below 150nm.
  • the method first synthesizes Ti(OH) 4 , metal-doped Ti(OH) 4 or metal-coated Ti(OH)4 in a solution, slurry, cake or dry powder form, and then places one of the foregoing into a closed reactor.
  • crystalline TiO 2 , metal-doped TiO 2 or metal-coated TiO 2 is synthesized from the Ti(OH) 4 , metal-doped Ti(OH) 4 or metal-coated Ti(OH) 4 , respectively, by heat treatment at a temperature above 10O 0 C under a pressure at or above the saturated vapor pressure of water.
  • the pressure in the closed reactor is achieved by water vapor pressure generated inside the reactor, water vapor pressure applied from outside the reactor, gas supplied from outside the reactor, or a mixture thereof.
  • titanium tetrachloride, titanium trichloride, titaniumoxychloride and. titanium sulfate may be used as a titanium source, but the present invention is not limited to these titanium sources and may use any organic or inorganic substance or mixtures that can dissolve in water and form titanium ions or titanium ion complexes.
  • NaOH, KOH, and NH 4 OH may be used as the alkaline substance, but the present invention is not so limited and may use any alkaline substance that can dissolve in water and increase the pH of the solution.
  • Educed Ti(OH) 4 undergoes several water cleaning processes using a centrifuge and ultrafilter system to remove impure ions residing therein.
  • Water washed Ti(OH) 4 can be obtained in the form of a solution, slurry, cake or dry powder through a concentration and drying process.
  • Metal doped Ti(OH) 4 is obtained by putting one or more metal salts into the water-soluble titanium source.
  • the water-soluble metal ion and the titanium ion are co-precipitated by adding the alkaline substance to the solution in which the titanium and metal are dissolved, and then adjusting the pH of the solution to 4 or higher as described above.
  • the present invention may use, but is not limited to, titanium tetrachloride, titanium trichloride, titaniumoxychloride or titanium sulfate as a titanium source.
  • the present invention may use, but it is not limited to NaOH, KOH, and NH 4 OH as the alkaline substance.
  • Water soluble salts of Ag, Zn, Cu, V, Cr, Mn, Fe, Co, Ni, Ge, Mo, Ru, Rh, Pd, Sn, W, Pt, Au, Sr, Al, and Si can be used as the source of the metal ion, although the present invention is not limited thereto and all water soluble metal salts may be used as well.
  • Co- precipitated metal-doped Ti(OH) 4 undergoes several water cleaning processes by using a centrifuge and ultrafilter system to remove impure ions residing therein. As a result of assay for water-washed metal-doped Ti(OH) 4 educts, added metal ingredients were detected, which are believed to co-precipitate together with the Ti ion upon addition of an alkaline substance. Water-washed metal-doped Ti(OH) 4 can be obtained in the form of a solution, slurry, cake, and dry powder through the concentration and drying process described above.
  • titanium tetrachloride, titanium trichloride, titaniumoxychloride or titanium sulfate may be used as the titanium source, but the present invention is not limited thereto and may use all organic and inorganic substances or mixtures that can dissolve in water and form titanium ions or titanium complex ions.
  • NaOH, KOH, and NH 4 OH can be used as the alkaline substance, but the present invention is not limited thereto and may use all alkaline substances that can dissolve in water and increase the pH of the solution.
  • metal salts of a desired amount are added into the dispersed Ti(OH) 4 , it is aged for a time that exceeds 5 minutes. It is preferable that the aging be at a temperature below 10O 0 C.
  • Water soluble salts of Ag, Zn, Cu, V, Cr, Mn, Fe 1 Co, Ni, Ge, Mo, Ru, Rh, Pd, Sn, W, Pt, Au, Sr, Al, and Si may be used as the metal salts in the present invention, but the practice of the present invention is not limited thereto and may use all water soluble metal salts.
  • the educts undergo a water cleaning process of 2-3 times to remove impure ions, obtaining metal-coated Ti(OH) 4 thereby.
  • water-washed Ti(OH) 4 , metal-doped Ti(OH) 4 , and metal-coated Ti(OH) 4 can exist in the form of a solution, slurry, cake or dry powder according to its moisture content and concentration degree. Considering the need for production efficiency, it is desirable to opt for the form of cake or dry powder having high titanium content.
  • Some condensed water is absolutely necessary in the reactor to decrease the reaction temperature to ensure that amorphous TiO 2 becomes anatase TiO 2 and to prevent the yellow color change mentioned above.
  • the pressure may be supplied by water vapor from the reaction, water vapor introduced into the reactor from outside, a gas such as an inert gas, or a combination of the preceding.
  • cake or dried Ti(OH) 4 was put into a closed reactor under the condition of removed humidity, and then it was reacted for 2 hours at 160°C by adding nitrogen having a pressure corresponding to the saturated vapor pressure. The phase obtained thereby was non-crystalline and it manifested a yellow color.
  • Titanium oxychloride ((dissolved TiCU in H 2 O by approximately 50 wt%)) was put into distilled water of 1 ,560cc. The final pH was adjusted to 6.5 by adding ammonia water after titanium oxychloride was completely dissolved. Then impure ions were removed by washing the educts with water. The Ti(OH) 4 with impure ions removed was then concentrated using a filtering system and it was dried for 12 hours at 6O 0 C. After dried specimen was put into the closed reactor and the pressure of the closed reactor was adjusted to 0.83 * 10 6 N/m 2 with argon gas, it was reacted for 2 hours at 16O 0 C.
  • Crystalline phase Ag-coated Ti ⁇ 2 having a primary particle size of approximately 10nm was formed (See Figs. 4(a) and (b)). It was verified that silver exists in the form of pure silver or silver oxide (See Figs. 4(c) and (d)).

Abstract

L’invention décrit un procédé pour la synthèse de TiO2, de TiO2 dopé par un métal, et de particules de TiO2 revêtues d’un métal de forme sphérique et de type aiguille dont la taille moyenne des particules est inférieure à 150 nm. Le procédé de l’invention consiste à synthétiser du Ti(OH)4, du Ti(OH)4 dopé par un métal ou du Ti(OH)4 revêtu par un métal, et à le faire réagir en appliquant une pression supérieure à la pression de la vapeur saturante à une température supérieure à 100 °C. La pression est obtenue à l’aide de la pression de la vapeur générée au cours de la réaction à l’intérieur d’un réacteur fermé, par de la pression appliquée de l’extérieur, ou d’un mélange des deux. Les gaz utilisés pour augmenter la pression de l’extérieur sont de préférence des gaz inertes tels que l’Ar et le N2 mais ne se limitent pas à des gaz inertes.
EP05807465A 2004-10-14 2005-10-13 Procede pour la synthese de nanoparticules de dioxyde de titane Withdrawn EP1812348A4 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US61878104P 2004-10-14 2004-10-14
PCT/US2005/036745 WO2006044495A1 (fr) 2004-10-14 2005-10-13 Procede pour la synthese de nanoparticules de dioxyde de titane

Publications (2)

Publication Number Publication Date
EP1812348A1 true EP1812348A1 (fr) 2007-08-01
EP1812348A4 EP1812348A4 (fr) 2009-12-23

Family

ID=36203288

Family Applications (1)

Application Number Title Priority Date Filing Date
EP05807465A Withdrawn EP1812348A4 (fr) 2004-10-14 2005-10-13 Procede pour la synthese de nanoparticules de dioxyde de titane

Country Status (6)

Country Link
US (1) US20080064592A1 (fr)
EP (1) EP1812348A4 (fr)
JP (1) JP2008516880A (fr)
KR (1) KR100869666B1 (fr)
CN (1) CN101065325B (fr)
WO (1) WO2006044495A1 (fr)

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CN102515269A (zh) * 2011-11-25 2012-06-27 黑龙江大学 水热法制备高活性多孔纳米晶二氧化钛光催化剂的方法
CN103055840B (zh) * 2012-12-06 2014-10-01 上海纳米技术及应用国家工程研究中心有限公司 超临界二氧化碳法制备稀土掺杂纳米二氧化钛光催化剂的方法及装置
CN104925750B (zh) * 2015-05-07 2017-01-04 南京文钧医疗科技有限公司 一种具有Yolk-Shell结构的TiO2纳米线-Ag/AgCl-Fe3O4复合材料的制备方法
CN106006726B (zh) * 2016-05-03 2018-11-27 广东风华高新科技股份有限公司 掺杂锐钛矿二氧化钛材料、其制备方法及其应用
CN113896235B (zh) * 2020-07-06 2023-09-26 宁波极微纳新材料科技有限公司 一种单分散纳米二氧化钛的制备方法及装置
CN113896230B (zh) * 2020-07-06 2024-02-06 极微纳(福建)新材料科技有限公司 一种提升二氧化钛分散性的方法
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CN113896233B (zh) * 2020-07-06 2024-02-09 极微纳(福建)新材料科技有限公司 一种低温晶化二氧化钛的方法

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